Scribd
Upload
9 views

Batch Distillation

Uploaded by

mudit
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
9 views

Batch Distillation

Uploaded by

mudit
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
You are on page 1/ 3

INDIAN INSTITUTE OF TECHNOLOGY KANPUR

Department of Chemical Engineering


Unit Operation Lab

Experiments Name: Batch Distillation

1. Scope:
When a liquid is to be separated into its components batch distillationis especially us
eful for small amount of material . A given batch distillation unitmay be used to
process many different mixtures. When there are several compounds (N) in the feed, one
batch column will suffice to separate all of them whereas N-1 continuous stills will be
required. When solids are present, batch distillation is moreconvenient than the
continuous one.

2. Objective:
(a) To observe the operation of batch distillation
(b) To determine the number o theoretical plates; to obtain an overall heat Balance.

3. Theory & Formulae:


In batch distillation, a batch of liquid is charged in the still and heated, and when
vaporshave reached the condensing system a portion of the condensed distillate is returned as
reflux. As top product take off is carried out , the material in the still becomes poorer in the
more volatile component (s) ,hence as the distillation proceeds the reflux ratio must be
increased to maintain the top-product quality, or sacrifice in sharpness of separation must be
made.
If the column is operated with a given mixture at total reflux, the
Fenske Underwood equation can be used to calculate theoretical plates for a binary
separation.
x p (1 − x s )
log
x s (1 − x p )
N +1 = (1)
log 

Where, α = Relative volatility


N = Theoretical plates
xp = Product concentration .
xs = Final still concentration ,mole fraction.

If the column is operated at a fixed know reflux ratio, then the product concentration varies
during the cycle. The variation of product concentration with amount of liquid remaining in
the still is given by
1
xs
S1 dxs
ln = 
S 2 x s ( x p − xs ) (2)
2

Where, S1= initial batch charge, moles


S2=residue in kettle at the end, moles
Relation betweenxp&xs can be obtained from X-Y diagram by plottingenriching section
operating line of slope determines by the fixed (L/V)ratio, with the lower terminus starting
with the initial still concentration and final line terminating with xs2. Based upon the
fixed no. of plates a relation between xp&xs can be calculated by the above procedure.
Equations (2) can then be integrated to give curves showing product and still composition
as functions of the percent of charge distilled.
(refer Perry’s Chemical Engineering Handbook,6th edition pg.13-82 to 13-85)

4. Materials and Apparatus:


The binary system used in the distillation experiment is ethanol-water. Analysis is carried out
by refractometer. The calibration curve of refractive index vs percent ethanol (0-100 %) must
be obtained at room temperature before hand. The reflux ratio can be adjusted by timer.
Other apparatus include sample bottles, thermometers or thermocouples.

5. Procedure:
5.1 Obtain the calibration curve for refractive index vs percent ethanol.
5.2 Charge a known amount of ethanol and water (50-50%) mixture in the still and start
heating.
5.3 Operate under total reflux (keeping the timer off) until steady state is reached obtained
distillate and bottoms (xp, xs) samples.
5.4 Take the necessary data – refractive index and specific gravityof reflux and residue,
cooling water rate, reflux rate and temperatureof inlet and outlet water stream in order
to be able to obtained a heat balance.
5.5 Record the weight (or volume) distilled vs time and record the weight of the still
sample.
5.6 Operate under a known fixed reflux ratio (say 5:1). Obtain samples at various times and
measure total amount of distillate collected.
5.7 Obtain RI and Specific Gravity of both Distillate collected and RI of bottoms.
5.8 Record the temperature of bottoms and distillate for heat balance.
5.8 Repeattherun at other known reflux ratio.

6. Results:
6.1 Plot calibration curve and equilibrium data for ethanol water system at 1.013 x 102
KN/m2total pressure.
6.2 Find number of theoretical stages using Fenske-Underhood equation and compare with
actual number of stages.
6.3 Set up material and energy balance equations.
6.4 Make a heat balance for the total reflux run and determine the % heat loss.
6.5 Plot moles of liquid remaining in the still vs distillate composition (s2vsxp) and compare
with results obtained from equation (2).
6.6 Comment on the sieve plates in the column.
6.7 Obtain a material balance on the last run and determine the % ethanol loss. Account for
all the ethanol.
7. Questions:
7.1 While setting up the equations, negligible column hold up is assumed. What happens if
the hold up is not actually negligible?
7.2 Can a packed column be used instead of sieve plate or bubble plate column for any
separation?
7.3 What must be done to maintain the distillate quality in a batch distillation column?
7.4 How will you set up the performance equation for the still if the assumption of constant
rate of distillate is not valid?
8. References:
8.1 Fenske, Ind.Eng.Chem. 24, 482, (1932)
8.2 Smoker & Rose, Trans Am.Inst.Chem.Engrs. 36, 285 (1940)
8.3 M. Van Winkle, “Distillation”, McGrow Hill Book Co. New York, (1967)
8.4 Perry’s Chemical Engineering Handbook,6th edition, Editors:RobertH.Perry and Don
Green.

You might also like